Method and apparatus for conveying liquids to be analyzed to an automatic spectrophotometrical reading cuvette

ABSTRACT

Method and apparatus for carrying out spectrophotometrical and colormetrical tests, wherein by a syringe a first predetermined amount of liquid is drawn from a first container and introduced into a second analysis container, and then ejected by a vacuum pump to wash said second container, then by said syringe a second metered amount of liquid for test operations is introduced into said second container, then ejecting the analyzed liquid by said vacuum pump. The apparatus comprises means for continuous cyclic operation, for enabling at a desired time the measuring means for the measures to be carried out.

United States Patent Vicario e 1 Dec. 12, 1972 [54] METHOD AND APPARATUS FOR CONVEYING LIQUIDS TO BE ANALYZED TO AN AUTOMATIC SPECTROPHOTOMETRICAL READING CUVETTE Guido Vicario, Piazza Guilio Cesare, Milan, Italy Filed: Feb. 5, 1971 Appl. No.: 112,860

Inventor:

us. c1. ..356/180 1111. c1. ..G0lj 3/46 Field of Search ..356ll80, 181, 173

[56] References Cited UNITED STATES PATENTS 3,401,591 9/1968 Anthon ..356/l81 Primary Examiner-Ronald L. Wibert Assistant Examiner-Conrad Clark Attorney-Christen & Sabol [57] ABSTRACT Method and apparatus for carrying out spectrophotometrical and colormetrical tests, wherein by a syringe a first predetermined amount of liquid is drawn from a first container and introduced into a second analysis container, and then ejected by a vacuum pump to wash said second container, then by said syringe a second metered amount of liquid for test operations is introduced into said second container, then ejecting the analyzed liquid by said vacuum pump. The apparatus comprises means for continuous cyclic operation, for enabling at a desired time the measuring means for the measures to be carried out.

9 Claims, 1 Drawing Figure i llllllllllll illlllll" METHOD AND APPARATUS FOR CONVEYING I LIQUIDS TO BE ANALYZED TO AN-AUTOMATIC. SPECTROPHOTOMETRICAL READING CUVETTE This invention relates to a method and apparatus capable of automatically carrying apredeterrninable amount of any liquid from a first container of any size, hereinafter referred to as test-tube, to another container generally comprising anautomatic three-way cu.- vette, having such physical shape and-characteristics as to be capable of carrying out spectrophotometrical and colormetrical tests on the liquid therein contained, and also successively automatically ejecting the sucked liquid from the cuvette, conveying it to athirdexhaust container.

The apparatus is characterized. by aflexible tube system of acid resistant material, the liquid: to be analyzed passing therethrough, and interconnecting; a

known three way, spectrophotometrical. cuvette, a. known glass calibrated syringeandassociatedpiston, a, valve controllably opened and. closed for'exhausting' the hydraulic circuits, an electromechanical control for automatically controlling said syringe. and. valve, a.

known power drivenvacuum pump sucking airffrom a hermetically sealed container referred to as flask, within which, upon evacuation, the-liquid will: exhaust on analysis completion through a conduit fromsaidcuvette.

The various steps of the process as provided by'the above described apparatus are as follows; transferring to the reading ,cuvette from the test-tubeforaportion of the liquid therein containedas predeterminediby the.

calibration of asyringe in order towash the three-way cuvette interior from the residual liquid previously tested'and to avoid contamination errors; ejecting the liquid contained in' the cuvette by suction; repeatedly transferring to the cuvette from the test-tube. fora second portion of liquid identical to thefirst portion and designed to be tested; signalling the spectrophotometrical reading systems about liquid transfer occurrence and then an interval for; analysis, accomplishment; finally ejecting the tested'liquid from thecuvette still .by suction.

The novel inventive concept consists of the principle.

for sucking and conveying from a test-tube. to an'automatic cuvette for spectrophotometrical chemical analyses metered liquid volumes through a syringe pro-- grammed by an electromechanical control; and also successively rapidly ejecting the liquid, on whichv the photometrical analyses have been carried out, through a flask and vacuum pump system.

Thus, the syringe sucks only the required'amount' of liquid, whereas the vacuum-pump is not equally reliably controllable and in case. of malfunction would'exhibit the risk of sucking in a momentall the liquid from the test-tube and scatter it. Conversely, thev exhaust is current flowing through these contacts when shorted by the disc sections 3 and 3" andbeingthe'flow shut off at the cable- 7, 7 between said two disc sections3 and 3',,the wiping contact being.connecteditoaterminal of motor 1 and. contact 5 directlyv connected to said electric power source. By shorting said laminar contacts Sand 5., a.pushbutton 55' enables to directly connect motor-1 to the power source'to'start' the operation of the apparatus, as it will be explained in the following. Through the rotation of its shaft 2", said motor I also controls. a. second. set of contacts, comprising: aconductive discsection 8 secured tothe insulating bearing 9'and the wipingcontacts 10 and: 10 carriedby the insulating bearing 11. Said contacts 10 and 10' are directly connected to the amplifier'35. of a measuring devicefor' enabling said measuring to=becarried out.

Fast with the driveshaft 2, on the central plane of the apparatus there are: a metal cam 12 operating by its profile and. a suitable follower 37 a liquid. valve 13 (shown'in: a sectionalview'); a handle 14' isalso connected tosaid shaft 2, while at l6=one end of apiston rod IS'is pivoted to'this handlel4, theother endof the piston rod .beingpivotedat '17 on a slide 18 free to run in two. guides 19, the slideandiguides beingmade of metal. material. A fork 20 is'secured" on saidslide 18.

andencloses the metal stem 21 of aprogrammed syringe-22. Outside the syringe, the metal: stem 21 carries two cylindricalblock'23 and23' freely slidable relative to said stem, but susceptible ofbeing clamped at any desired position throughascrew- 24- and 24', respectively, andin additiontheend of stem21 inside of the syringe 22 is inserted and'blocked in a piston 25 of acid resistant material, sliding within said syringe 22', the tight sealing bet ween said piston andsyringe being ensured by a gasket or ring 26. (shown in a sectional view), inserted in aproper peripheral groove in the piston 25;

Motor 1, guides 19; syringe221andvalve13 are all members which are secured on a metal rigid support, not-shown in the drawing.

A known" automatic cuvette 27 is outside the apparatus and is made of acid resistant material; therein'a suitably'sized chamber 28 isformed and'provided'. on the front wall, and .rear wall correspondingly, with two suitable apertures or-windows 29 of transparent material for'the passage therethrough of light beams from the light source 3.3. The hollow may be filled with liquid to beanalyzed through conduits 30'and 31 and completely exhausted through conduit 32. Thus, as shownin the accompanying drawing, conduit 30 is connected to syringe 22 by theflexiblehose 30', conduit 31 is connected by the flexible hose'3l' to probe 46 which is inserted into the tube-test 4Tcontaining the liquid to be analyzed and conduit 32 is connected by the flexible hose 32 to the inlet of valve 13, the outlet of which is connected in turn by the flexible hose or conduit to the container or flask 48,

Through the two apertures or windows 29 in the cuvette 27, the spacing and size of which are known, the spectrophotometrical and colorrnetrical measuring is carried out by means of the light from said source 33, this light being in a per se known manner sensed by the photodetector 34 which applies a signal to the amplifier 35, the outlet of which is connected in turn to the measuring meter 36. As shown in the drawing, said valve 13 comprises a cylindrical shaft or follower 37, carrying at its extreme end a roller 38, which is retained by a pin and rotates following the profile of cam 12. The shaft 37 is also secured to a piston 39 of acid resistant material sliding within a cylindrical chamber 40 in the body of valve 13.

As shown in a sectional view in the drawing, said cylindrical piston 39 on being urged by the follower 37 will press against the gasket or seal 41 positioned between the cover 42 and the body of valve 13, thus preventing the liquid from passing from conduit 32' to conduit 45; liquid sealing against shaft 37 is ensured by a ring seal or gasket 43 of acid resistant material seated within a groove on piston 39, while a spring 57 is effective for maintaining the roller 38 of follower 37 always adhering to the profile of cam 12.

The withdrawal probe 46 is outside the apparatus and comprises a thin tube of acid resistant material connected to the reading cuvette 27. The test-tube 47 is an acid resistant container of any type; similarly, the flask 48 is a known device comprising a hermetically sealed container and is connected through the flexible hose 44 to the inlet of the vacuum pump 50, the latter being also a known device. Pump 50 is driven by a motor which through a piston rod cam device 51 is connected to a piston 52 which on reciprocating within the chamber 53 and through the opening or closing of valves 54 and 54' causes the air in the flask 48 to be sucked and delivered to the outside; when valve 13 is closed, vacuum will be provided in the flask 48.

The transfer of predetermined liquid volumes to the cuvette and associated reading are as follows:

The probe 46 is manually immersed into the testtube 47, then the push-button 55 is depressed for a moment and because of being supplied the motor 1 starts to rotate driving the members connected thereto; during this rotation the sector 3, on shorting the contacts and 5', will ensure a supply for motor 1 until the latter has rotated the shaft 2 by 180. After rotation by 180, the wiping contacts will be at hollow 7, thus breaking the circuit.

During the motor rotation, said shaft 2 will drive the cam 12, but without any change in the position of valve 13 which remains closed, the cam profile being unaltered through 180. The shaft 2 also drives the handle 14 causing with lever the slide 18 to move downwards, this slide through the fork interposed between the stops 23 and 23' downward moving the stem 21 and the piston of syringe 22.

By moving down the syringe 22, said piston 25 will provide for drawing some amount of liquid from the test-tube 47 which, through the probe 46, is supplied to the chamber 28 of cuvette 27 to complete filling up due to the location of the sucking conduit which is at the top of said chamber 28. Of course, the volume of syringe 22 will be adjusted, by adjusting said stops 23 and 23' for sucking a same volume as that of chamber 28 of cuvette 27, probe 46 and its associated conduit 31 Thus, the first cycle is completed. By depressing the pushbutton 55 a second time, the motor 1 will be again supplied and its shaft 2 will again rotate by In this second cycle, as the cam 12 presents its relieved profile, valve 13 will be opened and because of spring 57 being effective on shaft 37, the probe 46 will have to be raised from the test-tube 47. On opening of valve 13, all of the liquid in the cuvette 27 and conduits 46 and 44 will be exhausted into the flask 48, as drawn by the vacuum provided therein by the vacuum pump 50. Further, due to operation of handle 14 and lever 15, the piston 25 of syringe 22 will be moved back to the starting position and the residual liquid in conduit 30, if any, will be ejected and sucked or drawn by said flask 48.

These first two sucking and exhausting cycles are employed for removing any residual of a previous analyzed liquid which would lead to an uncorrect spectrophotometrical reading. However, the volume being transferred should be the minimum useful for washing and reading operations in order not to waste an undue portion of sample and to this end the sucking mechanism comprises an adjustable syringe.

Now the device will be capable of repeating again the first cycle and thus by depressing again said pushbutton 55 and introducing the probe 46 into the test-tube 47 the liquid will be transferred again to the cuvette 27 At the completion of this cycle, the sector 8, which is driven by a pair of gears 60 and 61 in a ratio of l :2, will short the wiping contacts 11 and 11' and, since these contacts are electrically connected to the amplifier 35 of the photometrical system, they will enable for measuring being carried out, and this device provides that the photometer can carry out its operationsonly on a completely stationary liquid.

The invention is particularly designed for chemical and biochemical laboratories.

What is claimed is:

1. Method for transferring a predetermined amount of sample liquid to be analyzed form a sample container to a closed cuvette chamber for carrying out spectrophotometrical and colorimetrical tests therein, comprising the steps of placing the interior of the cuvette chamber in communication with a probe and a syringe pump having a pressure stroke and a suction stroke, inserting said probe into said sample liquid in the sample container, withdrawing a predetermined amount of sample from the sample container and transferring said withdrawn sample to the cuvette chamber by actuating a suction stroke of said syringe pump to reduce the pressure in said chamber by a predetermined magnitude, removing the probe from the sample liquid, establishing communication between the botuse in tom of said cuvette chamber and a source of vacuum to withdraw all of the liquid in the cuvette chamber, cutting off said communication between the cuvette chamber and vacuum source, and again withdrawing sample and transferring withdrawn sample to the cuvette chamber by actuating a suction stroke of the syringe pump while the probe is inserted in the sample liquid.

2. Method defined in claim 1, which includes the step of simultaneously actuating a pressure stroke of said syringe pump while said source of vacuum is in communication with the cuvette chamber.

3. Apparatus for carrying out spectrophotometrical and colorimetrical tests on successive samples of liquids, comprising a closed cuvette chamber having portions of opposing walls provided with means to permit transmission of radiant energy through a liquid contained therein, photodetector means including measuring means positioned to be responsive to radiant energy transmitted through said contained liquid, probe means to be inserted into a liquid to be sampled, reversible syringe pump means having a reciprocating piston, conduit means connecting said probe means and said syringe pump means in communication with the interior of said cuvette chamber to transfer liquid from a sample liquid container into said cuvette chamber when the probe means is inserted in said sample liquid and said syringe piston is moved in one direction to create suction in said conduit means and cuvette chamber, vacuum pump means, outlet conduit means including valve means having an open and a closed position and a closed flask connecting said vacuum pump means with the bottom of the interior of said cuvette chamber to withdraw all of the liquid from said cuvette chamber when said valve means is in said open position, electric motor means to reciprocate said syringe means piston, and switching means to connect said motor means with a source of energy, said switching means including means to maintain said valve means closed when said piston is moved by the motor means said suction stroke to maintain said valve means open when said piston is moved in the opposite direction and to energize said measuring means at a predetermined position of said piston.

4. Apparatus as defined in claim 3, wherein said electric motor means includes a rotary driving shaft, a reciprocable slide, crank linkage means connecting said rotary shaft and said slide, the piston of said syringe pump means including an elongated stem, and means connecting said slide with said stem to reciprocate said piston.

5. Apparatus as defined in claim 4, wherein said means connecting said slide with said stem includes adjustment means to vary the stroke of said piston.

6. Apparatus as defined in claim 5, wherein said means connecting said slide with said stem includes a pair of stop blocks positioned on said stem in longitudinally spaced relation, and a fork connected to said slide to engage alternately with a respective one of said pair of stop blocks when the slide is reciprocated.

7. Apparatus as defined in claim 6, wherein each 0 said stop blocks is longitudinally adjustably positioned on said stem to permit adjustment of the stroke of the piston.

8. Apparatus as defined in claim 2, wherein said valve means included in said outlet conduit means comprises a cylindrical chamber closed at one end by a reciprocable valve piston, said chamber being provided with an inlet opening in communication with the interior of said cuvette chamber and an outlet opening in communication with said vacuum pump means, said valve piston being reciprocable between a first position to block communication between said inlet and outlet openings and a second position to allow communication between the inlet and outlet openings.

9. Apparatus as defined in claim 8, wherein said switching means includes rotary cam-and -follower means, and means connecting said electric motor means to rotate said cam, said follower means being connected with said valve piston to reciprocate said valve piston between said first and second positions.

UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTTN Patent No. 3,7 5 ,773 Dated December 12, 1972 Inventor) Guido V1car1o It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:

In the heading, after item [21], insert --[30] Foreign Application Priority Data, February 11, 1971, Italy In claim 8, line 1, change "2" to 3.

Signed and sealed this 27th day of March 1973.

(SEAL) Attest:

EDWARD M.FLETCHER,JR. ROBERT GOTTSCHALK Attesting Officer Commissioner of Patents FORM PO-IOSO (10-69) USCOMM-DC 60376-P69 US. GOVERNMENT PRINTING OFFICE: I969 0-366-334 

1. Method for transferring a predetermined amount of sample liquid to be analyzed form a sample container to a closed cuvette chamber for carrying out spectrophotometrical and colorimetrical tests therein, comprising the steps of placing the interior of the cuvette chamber in communication with a probe and a syringe pump having a pressure stroke and a suction stroke, inserting said probe into said sample liquid in the sample container, withdrawing a predetermined amount of sample from the sample container and transferring said withdrawn sample to the cuvette chamber by actuating a suction stroke of said syringe pump to reduce the pressure in said chamber by a predetermined magnitude, removing the probe from the sample liquid, establishing communication between the bottom of said cuvette chamber and a source of vacuum to withdraw all of the liquid in the cuvette chamber, cutting off said communication between the cuvette chamber and vacuum source, and again withdrawing sample and transferring withdrawn sample to the cuvette chamber by actuating a suction stroke of the syringe pump while the probe is inserted in the sample liquid.
 2. Method defined in claim 1, which includes the step of simultaneously actuating a pressure stroke of said syringe pump while said source of vacuum is in communication with the cuvette chamber.
 3. Apparatus for carrying out spectrophotometrical and colorimetrical tests on successive samples of liquids, comprising a closed cuvette chamber having portions of opposing walls provided with means to permit transmission of radiant energy through a liquid contained therein, photodetector means including measuring means positioned to be responsive to radiant energy transmitted through said contained liquid, probe means to be inserted into a liquid to be sampled, reversible syringe pump means having a reciprocating piston, conduit means connecting said probe means and said syringe pump means in communication with the interior of said cuvette chamber to transfer liquid from a sample liquid container into said cuvette chamber when the probe means is inserted in said sample liquid and said syringe piston is moved in one direction to create suction in said conduit means and cuvette chamber, vacuum pump means, outlet conduit means including valve means having an open and a closed position and a closed flask connecting said vacuum pump means with the bottom of the interior of said cuvette chamber to withdraw all of the liquid from said cuvette chamber when said valve means is in said open position, electric motor means to reciprocate said syringe means piston, and switching means to connect said motor means with a source of energy, said switching means including means to maintain said valve means closed when said piston is moved by the motor means said suction stroke to maintain said valve means open when said piston is moved in the opposite direction and to energize said measuring means at a predetermined position of said piston.
 4. Apparatus as defined in claim 3, wherein said electric motor means includes a rotary driving shaft, a reciprocable slide, crank linkage means connecting said rotary shaft and said slide, the piston of said syringe pump means including an elongated stem, and means connecting said slide with said stem to reciprocate said piston.
 5. Apparatus as defined in claim 4, wherein said means connecting said slide with said stem includes adjustment means to vary the stroke of said piston.
 6. Apparatus as defined in claim 5, wherein said means connecting said slide with said stem includes a pair of stop blocks positioned on said stem in longitudinally spaced relation, and a fork connected to said slide to engage alternately with a respective one of said pair of stop blocks when the slide is reciprocated.
 7. Apparatus as defined in claim 6, wherein each o said stop blocks is longitudinally adjustably positioned on said stem to permit adjustment of the stroke of the piston.
 8. Apparatus as defined in claim 2, wherein said valve means included in said outlet conduit means comprises a cylindrical chamber closed at one end by a reciprocable valve piston, said chamber being provided with an inlet opening in communication with the interior of said cuvette chamber and an outlet opening in communication with said vacuum pump means, said valve piston being reciprocable between a first position to block communication between said inlet and outlet openings and a second position to allow communication between the inlet and outlet openings.
 9. Apparatus as defined in claim 8, wherein said switching means includes rotary cam-and-follower means, and means connecting said electric motor means to rotate said cam, said follower means being connected with said valve piston to reciprocate said valve piston between said first and second positions. 